CN106467604A - A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof - Google Patents
A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof Download PDFInfo
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- CN106467604A CN106467604A CN201610896393.8A CN201610896393A CN106467604A CN 106467604 A CN106467604 A CN 106467604A CN 201610896393 A CN201610896393 A CN 201610896393A CN 106467604 A CN106467604 A CN 106467604A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof, it passes through water-based free radical copolyreaction by unsaturated polyether monomer, unsaturated acids anhydride monomer, the unsaturated carboxylic acid ester monomer of bifunctionality and unsaturated phosphate ester monomer with 1: 3: 0.05～0.5: 0.05～0.2 mol ratio and is obtained.The viscosity reduction type polycarboxylate water-reducer of the present invention not only has the advantages that water-reducing rate height, function of slump protection are good, is also effectively reduced the viscosity of concrete, improves concrete workability, and material is soft, and flow velocity is fast, improves the workability of concrete.
Description
Technical field
Present invention building additive technical field is and in particular to a kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof.
Background technology
Constantly expand with civil engineering scale, scientific and technological level improve constantly, some high-rise long spans, have specific function require
Important building emergence, such as construction of skyscraper, super-span bridge and huge water-control project etc. is it is desirable to coagulation
Soil must have higher intensity, more preferable durability, more excellent stability, and these demands facilitate concrete from common to height
Performance or even very-high performance direction are progressively developed.The raising of concrete strength is mainly realized by reducing water-cement ratio, and this also leads
Cause concrete viscosity larger, caused a series of construction problems such as concrete-agitating, transport, pumping, largely limit
The popularization of high-strength shale ceramsite and application.
How to reduce concrete viscosity becomes the key issue of high-strength shale ceramsite development.From high-strength strong with superelevation
From the point of view of the composition of concrete and preparation method, adoptable viscosity reducing process is mainly from organic admixture and admixture two at present
Aspect is carried out.The organic admixture adding is mainly air entraining agent, and the incorporation of air entraining agent makes formation in concrete mix micro- in a large number
The spherical bubble of little closing, these microbubbles, as ball, reduce the frictional resistance between particles of aggregates, thus reducing viscous
Degree, but air entraining agent viscosity reduction limited use, the bubble of introducing has a negative impact to the intensity of high-strength concrete, with regard to water reducer
Still unintelligible to the concrete viscosity mechanism of action.
CN103553413A discloses a kind of Viscosity-control type polycarboxylate water-reducer and preparation method thereof.This water reducer is not mainly with
Saturated species monomer, unsaturated polyoxyethylene monomer and tune allonge body (predominantly unsaturated alkyl ester, fluorinated ester, alkyl third
Acrylamide or its mixture) in 70～90 DEG C of aqueous solution copolymerization and obtain.This water reducer significantly reduces cement paste
Plastic viscosity, but need also exist for high temperature in process of production, and energy consumption is larger；Allonge body is most importantly adjusted need to be first dissolved in table
In the aqueous surfactant solutions of face, then participate in polyreaction, but these surfactants cannot remove in end product.Polycarboxylic acids are high
Performance water reducer originally belongs to air-entraining water-reducing agent, and surfactant is respectively provided with air-entraining function to varying degrees, therefore should
In application, product obtained by method is likely to result in that high-strength concrete air content is bigger than normal so as to intensity cannot ensure.
CN102643042A discloses a kind of cross-linking type polycarboxylate water-reducer.This water reducer is with methallyl alcohol polyoxy second
Alkene ether, polyethylene glycol dimethacrylate, methylpropene sodium sulfonate and acrylic acid in 60～62 DEG C of aqueous solution copolymerization and
?.This water reducer be mainly using polyethylene glycol dimethacrylate as cross-linking agent, using its ester bond under alkaline environment water
The principle that solution discharges polycarboxylic acids molecule plays the effect that the slump keeps.But it is being applied to the high-strength mixed of low water binder ratio
During solidifying soil, its effect is similar with the polycarboxylate water-reducer with polyethylene glycol monomethyl ethermethacrylic acid esters as side chain, and cannot be very
Good hydrolysis, keeps to the slump and fluidity；Simultaneously because the slump of methyl allyl polyoxyethylene ether keeps energy
Power is also limited, therefore this product also cannot really meet needs have superior fluidity can high-strength concrete require；And by
In raw material double bond activity with the reason initiator system, during polyreaction temperature required also higher it is impossible to realize low-temperature energy-saving.
Content of the invention
It is an object of the invention to overcoming prior art defect, provide a kind of viscosity reduction type polycarboxylate water-reducer.
Another object of the present invention is to providing the preparation method of above-mentioned viscosity reduction type polycarboxylate water-reducer.
Technical scheme is as follows：
A kind of viscosity reduction type polycarboxylate water-reducer, it is by unsaturated polyether monomer, unsaturated acids anhydride monomer, bifunctionality not
Saturated carboxylic acid ester monomer and unsaturated phosphate ester monomer are with 1: 3: 0.05～0.5: 0.05～0.2 mol ratio by aqueouss freely
Base copolyreaction is obtained, and unsaturated polyether monomer is 3- methyl-3- butene-1-polyoxyethylene ether, allyl polyethenoxy base
One of ether and 2- methacrylic polyoxyethylene ether or two kinds, unsaturated acids anhydride monomer is maleic anhydride, itaconic anhydride,
Fumaric acid acid anhydride, dimethyl maleic anhydride, crotonic anhydride, methacrylic acid, Citric anhydride or acrylic anhydride, unsaturated carboxylic acid
Ester monomer is 1,4-CHDM diacrylate, BDO diacrylate or neopentylglycol diacrylate,
Unsaturated phosphate ester monomer is di(2-ethylhexyl)phosphate (hydroxy ethyl) ester or phosphoric acid hydrogen two (methylacryoyloxyethyl) ester.
In a preferred embodiment of the invention, its weight average molecular weight is 20000～60000.
A kind of preparation method of above-mentioned viscosity reduction type polycarboxylate water-reducer, comprises the steps：
(1) unsaturated polyether monomer, unsaturated acids anhydride monomer and suitable quantity of water are added in reaction unit, stirring and dissolving；
(2) at 30～40 DEG C, disposable addition oxidizing agent solution in the material of step (1) gained, and be sufficiently stirred for；
(3) the unsaturated carboxylic acid ester monomer of difference Deca bifunctionality, unsaturated phosphoric acid in the material of step (2) gained
The mixed solution of ester monomer and chain-transferring agent and the aqueous solution of reducing agent, drip off in 2～4h, and after completion of dropwise addition, ripening is at least
1h, finally, adds the aqueous solution of sodium hydroxide to be neutralized, that is, obtains described viscosity reduction type polycarboxylate water-reducer.
In a preferred embodiment of the invention, described oxidant is hydrogen peroxide, Ammonium persulfate. or sodium peroxydisulfate.
In a preferred embodiment of the invention, described reducing agent be ascorbic acid, sodium sulfite, sodium peroxydisulfate or
2- hydroxyl -2- sulfinatoacetic acid dipotassium.
In a preferred embodiment of the invention, described chain-transferring agent is TGA, 3- mercaptopropionic acid, sulfydryl second
Alcohol or mercaprol.
It is further preferred that the consumption of described oxidant is the 2～5% of unsaturated polyether monomer mass, described reducing agent
Consumption be the 1～2.5% of unsaturated polyether monomer mass, the consumption of described chain-transferring agent is unsaturated polyether monomer mass
2～4%.
Beneficial effects of the present invention：
(1) the viscosity reduction type polycarboxylate water-reducer of the present invention not only has the advantages that water-reducing rate height, function of slump protection are good, also effectively
Ground reduces the viscosity of concrete, improves concrete workability, and material is soft, and flow velocity is fast, improves the workability of concrete.
(2) the preparation method process is simple of the viscosity reduction type polycarboxylate water-reducer of the present invention, convenient for production, and pollution is little.
Specific embodiment
Below by way of specific embodiment, technical scheme is further detailed and describes.
In following embodiments, the weight average molecular weight of obtained viscosity reduction type polycarboxylate water-reducer is 20000～60000, phase
Unsaturated polyether monomer, unsaturated acids anhydride monomer, the unsaturated carboxylic acid ester monomer of bifunctionality and the unsaturated phosphate ester list answered
The mol ratio of body is 1: 3: 0.05～0.5: 0.05～0.2.The consumption of oxidant is the 2～5% of unsaturated polyether monomer mass,
The consumption of reducing agent is the 1～2.5% of unsaturated polyether monomer mass, and the consumption of chain-transferring agent is unsaturated polyether monomer mass
2～4%.
Embodiment 1
(1) 100 parts of 3- methyl-3- butene-1-polyoxyethylene ether, 300 parts of maleic anhydride and water are added to instead
Answer in kettle, stirring makes it dissolve；
(2) at 30～40 DEG C, the disposable hydrogen peroxide solution adding 2 parts in the material of step (1) gained, and stir
Mix；
(3) in the material of step (2) gained respectively the 1,4-CHDM diacrylate of 0.2 part of Deca,
The water of the ascorbic acid of 0.05 part of di(2-ethylhexyl)phosphate (hydroxy ethyl) ester and 2 parts of the mixed solution of TGA and 1 part
Solution, 2～4h drips off, after completion of dropwise addition, ripening 1h, finally, add the aqueous solution (32%) of sodium hydroxide so as to neutralize, that is,
Obtain viscosity reduction type polycarboxylate water-reducer (50%) that described weight average molecular weight is 31000.
Embodiment 2
(1) 100 parts of allyl polyethenoxy base ether, 300 parts of itaconic anhydride and water are added in reactor, stirring
So that it is dissolved；
(2) at 30～40 DEG C, the disposable ammonium persulfate solution adding 4 parts in the material of step (1) gained, and stir
Mix；
(3) the BDO diacrylate of 0.3 part of Deca of difference, 0.1 part of phosphorus in the material of step (2) gained
The water of the sodium sulfite of the mixed solution of 3- mercaptopropionic acid of sour hydrogen two (methylacryoyloxyethyl) ester and 3 parts and 1.5 parts
Solution, 2～4h drips off, after completion of dropwise addition, ripening 1h, finally, add the aqueous solution (32%) of sodium hydroxide so as to neutralize, that is,
Obtain viscosity reduction type polycarboxylate water-reducer (50%) that described weight average molecular weight is 42500.
Embodiment 3
(1) 100 parts of 2- methacrylic polyoxyethylene ether, 300 parts of Citric anhydride and water are added to reactor
In, stirring makes it dissolve；
(2) at 30～40 DEG C, disposably add 5 parts of sodium peroxydisulfate solution in the material of step (1) gained, and stir
Mix；
(3) neopentylglycol diacrylate of 0.5 part of Deca of difference, 0.15 part of phosphorus in the material of step (2) gained
The aqueous solution of the sodium hypophosphite of the mixed solution of mercaptoethanol of sour hydrogen two (methylacryoyloxyethyl) ester and 4 parts and 2 parts,
2～4h drips off, after completion of dropwise addition, ripening 1h, and finally, add the aqueous solution (32%) of sodium hydroxide so as to neutralization, that is, obtain institute
State viscosity reduction type polycarboxylate water-reducer (50%) that weight average molecular weight is 50300.
Embodiment 4
(1) 100 parts of 3- methyl-3- butene-1-polyoxyethylene ether, 300 parts of dimethyl maleic anhydride and water are added
Enter in reactor, stirring makes it dissolve；
(2) at 30～40 DEG C, the disposable hydrogen peroxide solution adding 3 parts in the material of step (1) gained, and stir
Mix；
(3) the BDO diacrylate of 0.1 part of Deca of difference, 0.2 part of phosphorus in the material of step (2) gained
2- hydroxyl -2- sulfino the second of the mixed solution of mercaprol of sour two (hydroxy ethyl) esters and 2.5 parts and 2.5 parts
The aqueous solution of sour dipotassium, 2～4h drips off, after completion of dropwise addition, ripening 1h, finally, add the aqueous solution (32%) of sodium hydroxide, make
Its neutralization, that is, obtain viscosity reduction type polycarboxylate water-reducer (50%) that described weight average molecular weight is 28400.
The sample that embodiment 1 to 4 synthesis is obtained, using standard cement, volume presses cement quality 0.2%, according to
GB8076-2008《Concrete admixture》And JGJ281-2012《High-strength concrete application technology code》, survey its concrete initial
The slump and divergence and through when the slump and divergence, decay barrel emptying time and through when decay a barrel emptying time.Coagulation
Native match ratio is：Cement 430kg/m3, flyash (II level) 30kg/m3, breeze (S95) 90kg/m3, sand 700kg/m3, stone
(5-10mm)368kg/m3, stone (10-20mm) 682kg/m3, divergence controls in 650 ± 10mm, acquired results such as table 1 institute
Show.
Table 1 testing concrete performance result
As shown in Table 1, using the viscosity reduction type polycarboxylate water-reducer of present invention preparation, have that water-reducing rate is high, function of slump protection is good,
Workability is good, and material is soft, and flow velocity is fast, and the low advantage of viscosity shows that the viscosity reduction type polycarboxylate water-reducer of the present invention more effectively drops
Low concrete viscosity, improves the workability of concrete.
Those of ordinary skill in the art understand, when technical scheme changes in following ranges, remain able to
To same as the previously described embodiments or close technique effect, still fall within protection scope of the present invention：
A kind of viscosity reduction type polycarboxylate water-reducer, it is by unsaturated polyether monomer, unsaturated acids anhydride monomer, bifunctionality not
Saturated carboxylic acid ester monomer and unsaturated phosphate ester monomer are with 1: 3: 0.05～0.5: 0.05～0.2 mol ratio by aqueouss freely
Base copolyreaction is obtained, and unsaturated polyether monomer is 3- methyl-3- butene-1-polyoxyethylene ether, allyl polyethenoxy base
One of ether and 2- methacrylic polyoxyethylene ether or two kinds, unsaturated acids anhydride monomer is maleic anhydride, itaconic anhydride,
Fumaric acid acid anhydride, dimethyl maleic anhydride, crotonic anhydride, methacrylic acid, Citric anhydride or acrylic anhydride, unsaturated carboxylic acid
Ester monomer is 1,4-CHDM diacrylate, BDO diacrylate or neopentylglycol diacrylate,
Unsaturated phosphate ester monomer is di(2-ethylhexyl)phosphate (hydroxy ethyl) ester or phosphoric acid hydrogen two (methylacryoyloxyethyl) ester.
A kind of preparation method of above-mentioned viscosity reduction type polycarboxylate water-reducer, comprises the steps：
(1) unsaturated polyether monomer, unsaturated acids anhydride monomer and suitable quantity of water are added in reaction unit, stirring and dissolving；
(2) at 30～40 DEG C, disposable addition oxidizing agent solution in the material of step (1) gained, and be sufficiently stirred for；
(3) the unsaturated carboxylic acid ester monomer of difference Deca bifunctionality, unsaturated phosphoric acid in the material of step (2) gained
The mixed solution of ester monomer and chain-transferring agent and the aqueous solution of reducing agent, drip off in 2～4h, and after completion of dropwise addition, ripening is at least
1h, finally, adds the aqueous solution of sodium hydroxide to be neutralized, that is, obtains described viscosity reduction type polycarboxylate water-reducer.
Described oxidant is hydrogen peroxide, Ammonium persulfate. or sodium peroxydisulfate.Described reducing agent be ascorbic acid, sodium sulfite,
Sodium peroxydisulfate or 2- hydroxyl -2- sulfinatoacetic acid dipotassium.Described chain-transferring agent is TGA, 3- mercaptopropionic acid, sulfydryl second
Alcohol or mercaprol.
The above, only presently preferred embodiments of the present invention, therefore the scope of present invention enforcement can not be limited according to this, that is,
The equivalence changes made according to the scope of the claims of the present invention and description and modification, all should still belong in the range of the present invention covers.
Claims (7)
1. a kind of viscosity reduction type polycarboxylate water-reducer it is characterised in that：It is by unsaturated polyether monomer, unsaturated acids anhydride monomer, double
The unsaturated carboxylic acid ester monomer of degree of functionality and unsaturated phosphate ester monomer are led to 1: 3: 0.05～0.5: 0.05～0.2 mol ratio
Cross water-based free radical copolyreaction to be obtained, unsaturated polyether monomer is 3- methyl-3- butene-1-polyoxyethylene ether, pi-allyl
One of polyoxyethylene ether and 2- methacrylic polyoxyethylene ether or two kinds, unsaturated acids anhydride monomer is maleic acid
Acid anhydride, itaconic anhydride, fumaric acid acid anhydride, dimethyl maleic anhydride, crotonic anhydride, methacrylic acid, Citric anhydride or acrylic acid
Acid anhydride, unsaturated carboxylic acid ester monomer is 1,4-CHDM diacrylate, BDO diacrylate or new penta 2
Alcohol diacrylate, unsaturated phosphate ester monomer is di(2-ethylhexyl)phosphate (hydroxy ethyl) ester or phosphoric acid hydrogen two (methacryloxypropyl
Ethyl) ester.
2. as claimed in claim 1 a kind of viscosity reduction type polycarboxylate water-reducer it is characterised in that：Its weight average molecular weight is 20000
～60000.
3. the viscosity reduction type polycarboxylate water-reducer described in a kind of claim 1 or 2 preparation method it is characterised in that：Including as follows
Step：
(1) unsaturated polyether monomer, unsaturated acids anhydride monomer and suitable quantity of water are added in reaction unit, stirring and dissolving；
(2) at 30～40 DEG C, disposable addition oxidizing agent solution in the material of step (1) gained, and be sufficiently stirred for；
(3) the unsaturated carboxylic acid ester monomer of difference Deca bifunctionality, unsaturated phosphate ester list in the material of step (2) gained
The mixed solution of body and chain-transferring agent and the aqueous solution of reducing agent, drip off in 2～4h, after completion of dropwise addition, ripening at least 1h,
Afterwards, add the aqueous solution of sodium hydroxide to be neutralized, that is, obtain described viscosity reduction type polycarboxylate water-reducer.
4. preparation method as claimed in claim 3 it is characterised in that：Described oxidant is hydrogen peroxide, Ammonium persulfate. or over cure
Sour sodium.
5. preparation method as claimed in claim 3 it is characterised in that：Described reducing agent is ascorbic acid, sodium sulfite, over cure
Sour sodium or 2- hydroxyl -2- sulfinatoacetic acid dipotassium.
6. preparation method as claimed in claim 3 it is characterised in that：Described chain-transferring agent be TGA, 3- mercaptopropionic acid,
Mercaptoethanol or mercaprol.
7. the preparation method as described in any claim in claim 3 to 6 it is characterised in that：The consumption of described oxidant
For the 2～5% of unsaturated polyether monomer mass, the consumption of described reducing agent is the 1～2.5% of unsaturated polyether monomer mass,
The consumption of described chain-transferring agent is the 2～4% of unsaturated polyether monomer mass.
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| CN106883355A (en) * | 2017-03-28 | 2017-06-23 | 中建商品混凝土有限公司 | A kind of low entraining viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
| CN108864389A (en) * | 2018-07-27 | 2018-11-23 | 科之杰新材料集团有限公司 | A kind of preparation method of viscosity reduction type sulfamate water reducer |
| CN109721690A (en) * | 2019-01-25 | 2019-05-07 | 中建西部建设西南有限公司 | A kind of viscosity reduction type polycarboxylic acids high efficiency solid water-reducing agent and its preparation and application |
| CN110330603A (en) * | 2019-08-07 | 2019-10-15 | 贵州铁建恒发新材料科技股份有限公司 | A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
| CN110358021A (en) * | 2019-05-29 | 2019-10-22 | 科之杰新材料集团有限公司 | A kind of cross-linking type wet mixing mortar plasticity-maintaining agent and preparation method thereof |
| CN111019057A (en) * | 2019-12-06 | 2020-04-17 | 湖北工业大学 | Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
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| CN111620715A (en) * | 2020-04-24 | 2020-09-04 | 佳固士(浙江)新材料有限公司 | Water-based capillary crystalline concrete surface repairing reinforcing material and preparation method and application thereof |
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Application publication date: 20170301 |